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Hydrogen Peroxide → 4-(tert-Butyl)pyridine 1-Oxide

HRID 1506272
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HRID 1506272 반응식
[C:1]([C:5]1[CH:10]=[CH:9][N:8]=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[OH:11]O>C(O)(=O)C>[C:1]([C:5]1[CH:10]=[CH:9][N+:8]([O-:11])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2]
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참가 물질

4

반응물 2

HCID 784Hydrogen PeroxideHCID 198784-tert-Butylpyridine

생성물 1

HCID 1410394-(tert-Butyl)pyridine 1-Oxide수율 87%

시약·촉매·용매 1

HCID 176Acetic Acid촉매

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온도
80 °C

실험 절차

In a reaction flask, 4-(tert-butyl)pyridine (13.5 g, 99.8 mmol) was dissolved in 70 ml of acetic acid (1.29 mmol), and 30 ml of hydrogen peroxide (H2O2) (30%, 0.30 mol) was then slowly added to obtain a mixture. The mixture was heated to 80° C. for reaction for 24 hours, and the temperature was then slowly reduced to 20° C. The reaction flask was vacuum pumped to remove solvents from the mixture, followed by addition of a sodium hydroxide aqueous solution to adjust the pH of the mixture to 8. Next, the mixture was washed several times with dichloromethane and with deionized water to collect an organic layer, and the organic layer was dehydrated using sodium sulfate (Na2SO4). The solvent was then removed from the organic layer, followed by vacuum drying, thereby obtaining light yellow solids (13 g, 87% yield), which was Compound L4-1 having a chemical structure represented by

후처리

  1. customto obtain a mixture
  2. customwas then slowly reduced to 20° C
  3. customto remove solvents from the mixture
  4. additionfollowed by addition of a sodium hydroxide aqueous solution
  5. washNext, the mixture was washed several times with dichloromethane
  6. customwith deionized water to collect an organic layer
  7. customThe solvent was then removed from the organic layer
  8. customdrying

출처 및 근거

ORD 기록
ord-5251ba51da4d45d98fc84c7f354bed93
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09219237B1

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